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Method for extracting benzoquinone compound in lithospermum

An extraction method and compound technology, applied in quinone separation/purification, organic chemistry, etc., can solve the problems of low process yield, long time, environmental pollution, etc., and achieve simple process operation, improve work efficiency, and reduce column wall effect. Effect

Inactive Publication Date: 2013-05-29
SHANDONG ACAD OF CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

With traditional extraction methods and processes, the yield is low, the cost is high, the purity is low, and the quality is poor. Not only cannot the medicinal index be reached, but also the level of large-scale production cannot be formed. Some processes pollute the environment
If the cell tissue culture process is used, the investment is large, the difficulty is high, the time is long, and the output is low, and it will not be able to reach the mass production scale of the enterprise.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Coarsely pulverize the dried comfrey, weigh 100kg of the coarse powder, put it into an extraction tank, add No. 6 solvent gasoline equivalent to 5 times the weight of the original drug (500kg), heat and reflux for 2 hours, suction filter while it is hot, and store the filtrate; Add 400kg of No. 6 gasoline to the tank again, carry out heat reflux extraction for 2 hours, suction filter while it is hot, and store the extract in addition, so repeat the heat reflux extraction four times, and the four reflux times are respectively 2 hours, 2 hours, 1 hour, and 1 hour way. The extracts were stored separately for future use. Take 25kg of spherical reaming silica gel, and put it into an ultra-short and thick filter column at one time. A 200-mesh sieve is set at the bottom of the filter column, the diameter of the column is 50 cm, and the height is 100 cm. After leveling the surface of the silica gel, pass the above extraction solution through the column directly above the cent...

Embodiment 2

[0024] Coarsely crush the dried comfrey, weigh 100kg of the coarse powder, put it into an extraction tank, add petroleum ether equivalent to 7 times the weight of the original drug (boiling range 30-60°C), heat and reflux for 2 hours, suction filter while it is hot, and store the filtrate ; Then use the same method to reflux and extract four times, the amount of petroleum ether used each time is 500 kg, 400kg, 300 kg, 300 kg, 100kg, 100kg, and the time is 2 h, 2 h, 1 h, 1 h, 1 h , 1h, the extracts were stored separately. Take 10kg of spherical reaming silica gel and put it into an ultra-short and thick filter column at one time. A 200-mesh sieve is set at the bottom of the filter column, the diameter of the column is 100 cm, and the height is 100 cm. After leveling the surface of the silica gel, pass the above-mentioned extraction solution in the order of extraction, directly above the center of the silica gel surface layer at a flow rate of 3 liters / min / kg of silica gel, and...

Embodiment 3

[0026] Coarsely crush the dried comfrey, weigh 100kg of the coarse powder, put it into an extraction tank, add petroleum ether (boiling range 30-60°C) equivalent to 6 times the weight of the original drug, heat and reflux for 2 hours, suction filter while it is hot, and store the filtrate ; Then use the same method to reflux and extract four times, the amount of petroleum ether used each time is 6 kg, 4 kg, 4 kg, 3 kg, and the time is 2h, 2h, 1h, 1h. The extract obtained each time was stored separately. Take 20kg of spherical reaming silica gel, and put it into an ultra-short and thick filter column at one time. A 200-mesh sieve is set at the bottom of the filter column, the diameter of the column is 65 cm, and the height is 100 cm. After leveling the surface of the silica gel, put the above-mentioned extraction solution in the order of extraction, and pass through the column directly above the center of the silica gel surface layer at a flow rate of 4 liters / min / kg of silica...

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PUM

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Abstract

The invention discloses a method for extracting a naphthoquinone compound in lithospermum, which comprises the following steps: crushing the lithospermum into coarse powders and adding a solvent for carrying out multiple reflux extraction, wherein total reflux time is not less than 6 hours; filtering mixed liquor obtained by reflux extraction while the mixed liquor is hot, respectively storing the extracting solution obtained by the reflux each time for standby application; injecting the extracting solutions into a chromatographic column which is internally provided with spherical chambering silica gel in accordance with an extraction sequence, and adsorbing ingredients in the extracting solutions; eluting the chromatographic column with an eluent and stopping the elution when the color of an effluent liquid is shallow or colorless; and concentrating and drying the eluted effluent liquid to obtain a lithospermum naphthoquinone compound coarse product. The method has simple process and operation and low cost; and the content of the naphthoquinone compound is more than 60%, thereby being suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for extracting effective components in comfrey, in particular to a method for extracting naphthoquinone compounds in comfrey. Background technique [0002] Comfrey is a perennial herb of the family Borganiaces, which was first recorded in "Shen Nong's Materia Medica", listed as a Chinese medicine, and its roots are used for medicine. It is bitter in taste, cold in nature, and returns to the liver meridian. It has the effects of cooling blood, promoting blood circulation, clearing away heat and detoxification, and is clinically used to treat blood heat and toxin excess, paralyzed rash purple and black, opaque measles, burns, and pimples. The comprehensive utilization of comfrey is quite extensive. At present, Chinese and foreign scientific and technological circles have realized the medicinal mechanism of comfrey. Studies have confirmed that shikonin is rich in shikonin and its derivatives, its content accounts for 3-6...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C46/10C07C50/32
Inventor 闫雪生徐新刚于蓓蓓付加雷
Owner SHANDONG ACAD OF CHINESE MEDICINE
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